HRID1197365

反应详情

EQUATION

反应方程式

HRID 1197365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A solution of 2,2-di-(benzylthiomethyl)pentan-1-ol (1.0 g Example XI) in dry dichloromethane (10 ml) was added to a stirred suspension of pyridinium chlorochromate (1.8 g) and anhydrous sodium acetate (0.11 g) in dry dichloromethane (25 ml) at 0° C., under a current of nitrogen. The reaction mixture was allowed to warm to 20° C. and then stirred for 2 hours. Dry diethyl ether was added and the mixture stirred for 30 minutes. The ethereal extracts were decanted off and the residue was washed with further portions of diethyl ether. The combined ethereal extracts were dried over anhydrous magnesium sulphate and the solvent was removed in vacuo. The residue was purified by chromatography on a mixture of silica and charcoal, eluting with diethyl ether. 2,2-Di(benzylthiomethyl)pentanal was obtained as a pale yellow oil (0.27 g).

WORKUP

后处理

  1. stirringthe mixture stirred for 30 minutes
  2. customThe ethereal extracts were decanted off
  3. washthe residue was washed with further portions of diethyl ether
  4. dry with materialThe combined ethereal extracts were dried over anhydrous magnesium sulphate
  5. customthe solvent was removed in vacuo
  6. customThe residue was purified by chromatography on a mixture of silica and charcoal
  7. washeluting with diethyl ether